US3810974A - Aluminum hydride preparation - Google Patents
Aluminum hydride preparation Download PDFInfo
- Publication number
- US3810974A US3810974A US00366933A US36693364A US3810974A US 3810974 A US3810974 A US 3810974A US 00366933 A US00366933 A US 00366933A US 36693364 A US36693364 A US 36693364A US 3810974 A US3810974 A US 3810974A
- Authority
- US
- United States
- Prior art keywords
- aluminum hydride
- ether
- distillation
- solution
- stable
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 title abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000000034 method Methods 0.000 abstract description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 46
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 238000004821 distillation Methods 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- LJWKFGGDMBPPAZ-UHFFFAOYSA-N ethoxyethane;toluene Chemical compound CCOCC.CC1=CC=CC=C1 LJWKFGGDMBPPAZ-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910010082 LiAlH Inorganic materials 0.000 description 3
- 239000003849 aromatic solvent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012280 lithium aluminium hydride Substances 0.000 description 3
- -1 lithium aluminum hydride Chemical compound 0.000 description 3
- 239000004449 solid propellant Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 235000010005 Catalpa ovata Nutrition 0.000 description 1
- 240000004528 Catalpa ovata Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- SPRIOUNJHPCKPV-UHFFFAOYSA-N hydridoaluminium Chemical compound [AlH] SPRIOUNJHPCKPV-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S149/00—Explosive and thermic compositions or charges
- Y10S149/12—High energy fuel compounds
Definitions
- Aluminum hydride is known to be useful as a fuel in solid propellants for rocket propulsion. Until recently aluminum hydride existed only in the form of an etherate and if any attempt was made to remove the ether by heating, the aluminum hydride decomposed.
- lithium aluminum hydride As indicated in the above reaction scheme, a one mole excess of lithium aluminum hydride is employed.
- the lithium chloride may be removed by any liquid-solid separation means such as decantation, centrifugation or filtration and the ether solution heated under vacuum .to produce stable aluminum hydride powder.
- Aluminum hydride in the form of a powder has very undesirable characteristics in the formation of a solid propellant.
- the powder tends to cake into lumps and even distribution of the aluminum hydride throughout the propellant is impossible. s
- the present invention resides in a method for recovering the aluminum hydride produced as disclosed in the reaction scheme discussed above, in which an improved crystalline form of aluminum hydride is recovered rather than the powdered form of the prior art as shown above.
- the precipitate of LiCl was allowed to settle and the supernatent solution was pumped by argon pressure througha glass wool filter into a one liter pressure equilibrated dropping funnel. This solution was then added to 3,400 ml. of toluene un-' der an argon-atmosphere. The ether-toluene solution was completely'free' of precipitate. The solution was added to a 5 liter round bottom flask fitted'with a stirrer, thermometer, a distillation head, and an electrically heated oil bath. The solvent was distilled according to the following schedule: 1
- benzene and xylene may also be used although the crystals of aluminum hydride obtained using benzene and xylene are less desirable.
- the procedure discussed above may be modified to obtain mono-crystalline chunks of aluminum hydride by carrying out the initial distillation step at a temperature between about 65 C. and about C. rather than at about 50C. to about 65 C.
- the distillation may be carried out between about 50 C. and about 65 C.
- the intermediate etherate forms and is converted to the stable aluminum hydride.
- the etherate form of aluminum hydride is bypassed and a stable form precipitates immediately. In this upper range even less decrepitation occurs and larger chunks of stable aluminum hydride are recovered.
- EXAMPLE 2 An ether solution of aluminum hydride was prepared as disclosed in Example 1 above. The solution was added to 3,400 ml. of toluene and the ether-toluene solution was distilled from a liter fiask equipped with a thermometer, stirrer, take-01f head and oil bath according to the following schedule:
- the flask was cooled and the contents transferred to a separatory funnel.
- the ether-toluene solution was withdrawn after the solid had settled.
- the solid was washed with 3 successive 500 ml. portions of ether and the ether was decanted until it remained clear during the washing.
- the product was then collected on a sintered glass filter and dried with an argon stream for one hour and then under vacuum overnight.
- the yield was a monocrystalline form of aluminum hydride in which the crystals were the size of about 30 to 50 microns in diameter.
- a large excess of solvent i.e. toluene, is employed in the distillation procedure-at least three, preferably at least five times the volume of the ether solution.
- the solvent is substantially dry, that is, contains less than about .1% water and preferably is even drier.
- the pressure and temperature at which distillation of the ether is conducted may vary, the important. feature being raising the temperature for conversion while about 8 to 10 percent of ether remains in solution.
- the pressure during distillation may vary from about 175 mm. Hg to about 500 mm. Hg, a lower pressure being required at lower temperatures, and during conversion preferably atmospheric pressure is employed.
- the temperature during distillation may vary from about 50 C. to about 85 C., and during conversion from about 90 C. to about 100 0.
- a process for producing aluminum hydride of an improved stable crystalline form comprising:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
THIS INVENTION RELATES TO A NOVEL FORM OF ALUMINUM HYDRIDE AND A METHOD FOR ITS PREPARATION.
Description
United States Pate-n1: once Mj'ilffiii 3,810,974 ALUMINUM HYDRIDE PREPARATION William M. King, Walnut, Calif., assignor to Aerojet- General Corporation, Azusa, Calif. No Drawing. Filed May 5, 1964, Ser. No. 366,933 Int. Cl. C01b 6/00 US. Cl. 423-645 Claims ABSTRACT OF THE DISCLOSURE This invention relates to a novel form of aluminum hydride and a method for its preparation.
Aluminum hydride is known to be useful as a fuel in solid propellants for rocket propulsion. Until recently aluminum hydride existed only in the form of an etherate and if any attempt was made to remove the ether by heating, the aluminum hydride decomposed.
A process has recently been developed for producing a stable form of aluminum hydride in the form of a fine powder. It was found that if an excess, preferably a one mole excess, of lithium aluminum hydride was utilized in the initial reactions, the ether solution in which the reac-' tion takes place may be removed under vacuum to obtain a stable form of aluminum hydride as a fine powder. The reaction scheme is indicated as follows:
As indicated in the above reaction scheme, a one mole excess of lithium aluminum hydride is employed. The lithium chloride may be removed by any liquid-solid separation means such as decantation, centrifugation or filtration and the ether solution heated under vacuum .to produce stable aluminum hydride powder.
Aluminum hydride in the form of a powder has very undesirable characteristics in the formation of a solid propellant. The powder tends to cake into lumps and even distribution of the aluminum hydride throughout the propellant is impossible. s
It is an object of the present invention to provide stable aluminum hydride in a crystalline form.
It is a further object of this invention to provide a prooess for the production of aluminum hydride in a crystalline form which is less reactive chemically, is thermally more stable and possesses superior physical characteristics for the production of solid propellants.
It has been known to recover aluminum hydride powder out of an ether-toluene solution containing excess lithium aluminum hydride by distillation at reduced pressure. This is accomplished by first precipitating out aluminum hydride etherate by distillation at about 50 C. to about 65 C. until only 3 to 5 percent of the ether remains in the toluene. This system is then brought up to atmospheric pressure, and the temperature is raised to about 90 to about 100 C. The aluminum hydride etherate is then converted to aluminum hydride powder after approximately 40 minutes at about 90 to about 100 C.
The present invention resides in a method for recovering the aluminum hydride produced as disclosed in the reaction scheme discussed above, in which an improved crystalline form of aluminum hydride is recovered rather than the powdered form of the prior art as shown above.
It has been found that the retention of 8 to 10 percent of the ether after the initial distillation step results in a superior final product. The retention of this other permits rearrangement of aluminum hydride during the conversion to the stable form of aluminum hydride. The decrepitation of the crystal is reduced and the final product is crystalline rather than the powder previously obtained. The chemical reactivity, thermal stability and bulk density are iiiiiiivd "062.111.; passage. estates passe-ed EXAMPLE 1 400 m1. of a 1 M solution of LiAlH in ether was added under an argon atmosphere to 100 ml. of 1 M AlCl in ether in a 1 liter graduated cylinder. The cylinder was stoppered and shaken to mix the contents. The precipitate of LiCl was allowed to settle and the supernatent solution was pumped by argon pressure througha glass wool filter into a one liter pressure equilibrated dropping funnel. This solution was then added to 3,400 ml. of toluene un-' der an argon-atmosphere. The ether-toluene solution was completely'free' of precipitate. The solutionwas added to a 5 liter round bottom flask fitted'with a stirrer, thermometer, a distillation head, and an electrically heated oil bath. The solvent was distilled according to the following schedule: 1
Pot Oil temp., temp., Pressure, Time, min. 0. 0. mm. Hg Remarks 100 200 Distillation begins. 59 75 200 Precipitation begins. 69 75 760 8-10 ether remains. 93 105 760 98 110 760 99 110 760 The flask was cooled to room temperature and the contents were transferred to a large separatory funnel and the solid was allowed to settle. The supernatent liquid was pumped out with argon pressure and the product was washed with three 500 ml. portions of dry ether. A final 500 ml. portion of dry ether was added and the suspension was filtered through a sintered glass filter attached to the bottom of the separatory funnel with a rubber stopper, using argon pressure through the funnel. The argon stream was continued for 1 hour to dry the product which was further dried in a vacuum desiccator overnight. Mono-crystalline particles ofaluminum hydride of the size up to aboutv 30 microns in diameterwere recovc red.
While the preparation of aluminum hydride was carried out in the example above using aluminum chloride,
it is well known that hydrogen chloride may be substituted for the aluminum chloride.
Although toluene is preferred as solvent for the distillation step, benzene and xylene may also be used although the crystals of aluminum hydride obtained using benzene and xylene are less desirable.
The procedure discussed above may be modified to obtain mono-crystalline chunks of aluminum hydride by carrying out the initial distillation step at a temperature between about 65 C. and about C. rather than at about 50C. to about 65 C.
The distillation may be carried out between about 50 C. and about 65 C. At the lower end of this range, on the order of about 50 C. to about 65 C. the intermediate etherate forms and is converted to the stable aluminum hydride. However, at the upper end of this range on the order of about 65 C. to about 85 C., the etherate form of aluminum hydride is bypassed and a stable form precipitates immediately. In this upper range even less decrepitation occurs and larger chunks of stable aluminum hydride are recovered.
EXAMPLE 2 An ether solution of aluminum hydride was prepared as disclosed in Example 1 above. The solution was added to 3,400 ml. of toluene and the ether-toluene solution was distilled from a liter fiask equipped with a thermometer, stirrer, take-01f head and oil bath according to the following schedule:
Pressure,
mm. Hg Remarks Distillation begins. Precipitation begins. 8-l0% ether remains.
The flask was cooled and the contents transferred to a separatory funnel. The ether-toluene solution was withdrawn after the solid had settled. The solid was washed with 3 successive 500 ml. portions of ether and the ether was decanted until it remained clear during the washing. The product was then collected on a sintered glass filter and dried with an argon stream for one hour and then under vacuum overnight. The yield was a monocrystalline form of aluminum hydride in which the crystals were the size of about 30 to 50 microns in diameter.
A large excess of solvent, i.e. toluene, is employed in the distillation procedure-at least three, preferably at least five times the volume of the ether solution. For best results the solvent is substantially dry, that is, contains less than about .1% water and preferably is even drier.
The pressure and temperature at which distillation of the ether is conducted may vary, the important. feature being raising the temperature for conversion while about 8 to 10 percent of ether remains in solution.
The pressure during distillation may vary from about 175 mm. Hg to about 500 mm. Hg, a lower pressure being required at lower temperatures, and during conversion preferably atmospheric pressure is employed.
The temperature during distillation may vary from about 50 C. to about 85 C., and during conversion from about 90 C. to about 100 0.
Having fully described the product, its method of preparation and its utilities, it is desired that the invention be limited only within the lawful scope of the appended claims.
I claim:
1. A process for producing aluminum hydride of an improved stable crystalline form, said process comprising:
(1) reacting AlCl with LiAlH; with the AlCl being present in one mole per about four moles of the LiAlH in an ether solvent to form an ether solution of AlH and a precipitate of LiCl (2) separating the LiCl precipitate from the ether solution;
(3) mixing the ether solution with an aromatic solvent, said aromatic solvent being present in at least three volumes per volume of ether solution, and carrying on a distillation under a subatmospheric pressure of about 175 mm. Hg to about 500 mm. Hg and ate temperature in the range of about C. to about 85 C. until the ether is present in the distillant in an amount of about 8 to about 10 percent;
(4) discontinuing the subatmospheric distillation and raising the temperature of the distillant to convert the aluminum hydride to a stable form; and
(5) recovering a stable aluminum hydride product.
2. A process in accordance with claim 1 wherein the aromatic solvent employed is toluene.
3. A process in accordance with claim 1 wherein 'the;v subatmospheric distillation is carried on at a temperature in the range of about 50 C. to about C.
4. A process in accordance with claim 1 wherein the subatmospheric distillation is carried on at a temperature in the range of about 65 C. to about C.
5. A process in accordance with claim 1 wherein the conversion to the stable aluminum hydride form is carried on at a temperature of about C. to about C.
1958 Germany 23204 OTHER REFERENCES Non-solvated Aluminum Hydride, Rice, Aug. 1, 1956, Technical Report to the Ofiice of Naval Research, Contract ONR494(04) pp. 1-5.
LELAND A. SEBASTIAN, Primary Examiner US. Cl. X.R. 149-109
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US00366933A US3810974A (en) | 1964-05-05 | 1964-05-05 | Aluminum hydride preparation |
| AU60785/73A AU6078573A (en) | 1964-05-05 | 1973-09-27 | Crystalline aluminium hydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US00366933A US3810974A (en) | 1964-05-05 | 1964-05-05 | Aluminum hydride preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3810974A true US3810974A (en) | 1974-05-14 |
Family
ID=23445211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00366933A Expired - Lifetime US3810974A (en) | 1964-05-05 | 1964-05-05 | Aluminum hydride preparation |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US3810974A (en) |
| AU (1) | AU6078573A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5670129A (en) * | 1994-12-24 | 1997-09-23 | Th. Goldschmidt Ag. | Method for synthesizing aluminum hydride |
| US6228338B1 (en) | 1999-06-16 | 2001-05-08 | Sri International | Preparation of aluminum hydride polymorphs, particularly stabilized α-alh3 |
| US20050222445A1 (en) * | 2004-04-05 | 2005-10-06 | Lund Gary K | Method for the production of alpha-alane |
| US20070066839A1 (en) * | 2004-04-05 | 2007-03-22 | Lund Gary K | Method for the production of alpha-alane |
| WO2013184617A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method of manufacturing alane including desolvation of an alane -etherate complex |
| WO2013184616A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method for preparation of alane-etherate and alane |
| WO2014058528A1 (en) | 2012-10-09 | 2014-04-17 | Intelligent Energy, Inc. | Method for preparation of crystalline alane using quaternary ammonium aluminum hydride |
| US9228267B1 (en) | 2011-11-07 | 2016-01-05 | Ardica Technologies, Inc. | Use of fluidized-bed electrode reactors for alane production |
| US9327974B1 (en) | 2011-11-07 | 2016-05-03 | Ardica Technologies, Inc. | Aluminum hydride production |
| US9550672B2 (en) | 2012-06-05 | 2017-01-24 | Intelligent Energy Inc. | Method for preparation of an alane-etherate complex and alane |
| US9676625B1 (en) | 2011-11-07 | 2017-06-13 | Ardica Technologies, Inc. | Synthesis of microcrystalline alpha alane |
| US10233079B2 (en) | 1999-06-16 | 2019-03-19 | Ardica Technologies, Inc. | Heating methods for aluminum hydride production |
| US10246785B2 (en) | 2011-11-07 | 2019-04-02 | Ardica Technologies, Inc. | Use of fluidized-bed electrode reactors for alane production |
| US10435297B2 (en) | 1999-06-16 | 2019-10-08 | Ardica Technologies, Inc. | Crystallization and stabilization in the synthesis of microcrystalline alpha alane |
-
1964
- 1964-05-05 US US00366933A patent/US3810974A/en not_active Expired - Lifetime
-
1973
- 1973-09-27 AU AU60785/73A patent/AU6078573A/en not_active Expired
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5670129A (en) * | 1994-12-24 | 1997-09-23 | Th. Goldschmidt Ag. | Method for synthesizing aluminum hydride |
| US6228338B1 (en) | 1999-06-16 | 2001-05-08 | Sri International | Preparation of aluminum hydride polymorphs, particularly stabilized α-alh3 |
| US6617064B2 (en) | 1999-06-16 | 2003-09-09 | Sri International | Stabilized aluminum hydride polymorphs |
| US10435297B2 (en) | 1999-06-16 | 2019-10-08 | Ardica Technologies, Inc. | Crystallization and stabilization in the synthesis of microcrystalline alpha alane |
| US10233079B2 (en) | 1999-06-16 | 2019-03-19 | Ardica Technologies, Inc. | Heating methods for aluminum hydride production |
| US20050222445A1 (en) * | 2004-04-05 | 2005-10-06 | Lund Gary K | Method for the production of alpha-alane |
| WO2005102919A1 (en) * | 2004-04-05 | 2005-11-03 | Alliant Techsystems, Inc. | METHOD FOR THE PRODUCTION OF α-ALANE |
| US6984746B2 (en) | 2004-04-05 | 2006-01-10 | Alliant Techsystems Inc. | Method for the production of α-alane |
| US20070066839A1 (en) * | 2004-04-05 | 2007-03-22 | Lund Gary K | Method for the production of alpha-alane |
| US7238336B2 (en) | 2004-04-05 | 2007-07-03 | Alliant Techsystems Inc. | Method for the production of α-alane |
| US9327974B1 (en) | 2011-11-07 | 2016-05-03 | Ardica Technologies, Inc. | Aluminum hydride production |
| US9228267B1 (en) | 2011-11-07 | 2016-01-05 | Ardica Technologies, Inc. | Use of fluidized-bed electrode reactors for alane production |
| US9676625B1 (en) | 2011-11-07 | 2017-06-13 | Ardica Technologies, Inc. | Synthesis of microcrystalline alpha alane |
| US10246785B2 (en) | 2011-11-07 | 2019-04-02 | Ardica Technologies, Inc. | Use of fluidized-bed electrode reactors for alane production |
| US9550672B2 (en) | 2012-06-05 | 2017-01-24 | Intelligent Energy Inc. | Method for preparation of an alane-etherate complex and alane |
| WO2013184616A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method for preparation of alane-etherate and alane |
| WO2013184617A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method of manufacturing alane including desolvation of an alane -etherate complex |
| WO2014058528A1 (en) | 2012-10-09 | 2014-04-17 | Intelligent Energy, Inc. | Method for preparation of crystalline alane using quaternary ammonium aluminum hydride |
Also Published As
| Publication number | Publication date |
|---|---|
| AU6078573A (en) | 1975-03-27 |
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